Acetic Anhydride → HCID 178473836, 화합물

HRID 1486594노트

반응식

HRID 1486594 반응식
F[C:2](F)(F)[C:3]([OH:5])=O.[Cl:8][C:9]1[CH:10]=[C:11]([NH:16][C:17]2[N:21]=[C:20]([NH:22][CH:23]3[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]3)[NH:19][N:18]=2)[CH:12]=[C:13]([Cl:15])[CH:14]=1.C(=O)(O)[O-].[Na+].C(OC(=O)C)(=O)C>C(#N)C>[Cl:15][C:13]1[CH:12]=[C:11]([NH:16][C:17]2[N:21]=[C:20]([NH:22][CH:23]3[CH2:28][CH2:27][N:26]([C:3](=[O:5])[CH3:2])[CH2:25][CH2:24]3)[NH:19][N:18]=2)[CH:10]=[C:9]([Cl:8])[CH:14]=1

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 178478184HCID 178478184, 화합물

생성물 1

HCID 178473836HCID 178473836, 화합물수율 84%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a stirred suspension of N3-(3,5-dichlorophenyl)-N5-(piperidin-4-yl)-1H-1,2,4-triazole-3,5-diamine 2,2,2-trifluoroacetate (50 mg, 0.113 mmol) in acetonitrile (5 mL), was added saturated sodium bicarbonate solution (5 mL) and acetic anhydride (14 mg, 0.136 mmol). The reaction mixture was stirred overnight at rt. The solution was extracted with EtOAc (3×10 mL) and dried with sodium sulfate. Removal of solvent gave the crude product, which was purified by flash chromatography to give 35 mg (84%) desired product as a white solid. MS +m/z: 369.0 (M+H)+

후처리

  1. extractionThe solution was extracted with EtOAc (3×10 mL)
  2. dry with materialdried with sodium sulfate
  3. customRemoval of solvent
  4. customgave the crude product, which
  5. customwas purified by flash chromatography

출처 및 근거

ORD 기록
ord-3a2caf15307d4b4381b6663471d222b8
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428469B2

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